📜四甲基二膦烷二硫化物置于氯化亚砜体系中,用93%的收率获得二甲基氯氧化磷 参考文献:Ramage,Robert; Atrash,Butrus; Hopton,David,Journal Of The Chemical Society. Perkin Transactions I,1985,P. 1217-1226 标题:Ramage,Robert; Atrash,Butrus; Hopton,David,Journal Of The Chemical Society. Perkin Transactions I,1985,P. 1217-1226
专利信息
专利号:US-7037691-B2 优先权日:2001-07-02 标题:Kinase mimic catalysts for asymmetric synthesis of phosphorylated inositols and cycloalkanols 发明人:MILLER SCOTT J; SCULIMBRENE BIANCA; MORGAN ADAM J 权利人:TRUSTEES BOSTON COLLEGE 摘要:The present invention provides peptide-based phosphorylation catalysts (PBPC's) for the asymmetric monophosphorylation of cyclitols, particularly myo-inositols. The PBPC's of the invention effect a regio and enantioselective phosphorylation of a myo-inositol in a manner analogous to enzymatic kinases, thereby functioning as effective “kinase mimics.â€? Although orders of magnitude less complex in terms of structure than macromolecular proteins, the PBPC's of the invention control product formation with high enantioselectivity (>98% ee). The synthetic (+)-myo-inositol-1-phosphate is optically and spectroscopically equivalent to naturally occuring compound. The ability of the low molecular weight PBPC's of the present invention to mimic stereoselective enzymes represents a powerful approach toward catalytic asymmetric synthesis of biologically important molecules, and for mechanistic modeling of biochemical transformations to enable their use in drug applications.
专利号:US-7189864-B2 优先权日:1990-11-19 标 题:Method of preparing intermediates useful in synthesis of retroviral protease inhibitors 发明人:NG JOHN S; PRZYBYLA CLAIRE A; MUELLER RICHARD A; VAZQUEZ MICHAEL L; GETMAN DANIEL P 权利人:SEARLE & CO 摘要:A synthesis is described for intermediates which are readily amenable to the large scale preparation of hydroxyethylurea-based chiral HIV protease inhibitors. The method includes forming a diastereoselective epoxide from a chiral alpha amino aldehyde.
专利号:US-6022996-A 优先权日:1990-11-19 标 题 :Method for making intermediates useful in synthesis of retroviral protease inhibitors 发明人:NG JOHN S; PRZYBYLA CLAIRE A; MUELLER RICHARD A; VAZQUEZ MICHAEL L; GETMAN DANIEL P 权利人:SEARLE & CO 摘要:A synthesis is described for intermediates which are readily amenable to the large scale preparation of hydroxyethylurea-based chiral HIV protease inhibitors. The method includes forming a diastereoselective epoxide from a chiral alpha amino aldehyde.
专利号:EP-0641333-B1 优先权日:1992-05-20 标 题 :Method for making intermediates useful in synthesis of retroviral protease inhibitors 发明人:NG JOHN S; PRZYBYLA CLAIRE A; MUELLER RICHARD A; VAZQUEZ MICHAEL L; GETMAN DANIEL P 权利人:SEARLE & CO; MONSANTO CO 摘要:A synthesis is described for intermediates which are readily amenable to the large scale preparation of hydroxyethylurea-based chiral HIV protease inhibitors. The method includes forming a diastereoselective epoxide compound of formula (I) from a chiral alpha amino aldehyde and halomethyllithium as an organometallic methylene-adding reagent. In formula (I) R<1> is selected from alkyl, aryl, cycloalkyl, cycloalkylalkyl and arylalkyl, which are optionally substituted with a group selected from alkyl, halogen, NO2, OR<9> or SR<9>, where R<9> represents hydrogen or alkyl; and P<1> and P<2> independently are selected from amine protecting groups, including but not limited to, arylalkyl, substituted arylalkyl, cycloalkenylalkyl and substituted cycloalkenylalkyl, allyl, substituted allyl, acyl, alkoxycarbonyl, aralkoxycarbonyl and silyl.
专利号:EP-0855388-B1 优先权日:1993-11-23 标 题 :Method for making intermediates useful in synthesis of retroviral protease inhibitors 发明人:NG JOHN S; PRZYBYLA CLAIRE A; MUELLER RICHARD A; VAZQUEZ MICHAEL L; GETMAN DANIEL P; FRESKOS JOHN J; DECRESCENZO GARY A; BERTENSHAW DEBORAH E; HEINTZ ROBERT M; ZHANG SUHONG; LIU CHIN; LANEMAN SCOTT A 权利人:SEARLE & CO 摘要:A synthesis is described for intermediates which are readily amenable to the large scale preparation of hydroxyethylurea-based chiral HIV protease inhibitors. The method includes forming a cyanohydrin from a chiral alpha amino aldehyde.
专利号:US-8722880-B2 优先权日:2012-08-22 标题:Method for preparing 42-(dimethylphosphinate) rapamycin 发明人:LEE KWANG-CHUNG; TUNG YEN-SHIH; LEE TZU-AI; SHIH YU-HSUAN 权利人:CHUNGHWA CHEMICAL SYNTHESIS & BIOTECH CO LTD; CHUNGHWA CHEMICAL SYNTHESIS & BIOTECH CO LTD 摘要:A method for preparing 42-(dimethylphosphinate) Rapamycin (Ridaforolimus) (I) is provided, which has advantages of high conversion rate and no 31,42-bis(dimethyl phosphinate) Rapamycin (III) generated. In the method of the present invention, Rapamycin (II) is firstly reacted with triethyl chlorosilane in a base condition to form 31,42-bis(triethylsilylether) Rapamycin (IV-b), followed by a selective deprotection process to obtain 31-triethylsilylether Rapamycin (V-b). Next, a phosphorylation reaction is performed by using dimethylphosphinic chloride under a base solution to obtain a crude product. Finally, a deprotection reaction is performed in a diluted sulfuric acid solution to obtain a crude product of Ridaforolimus (I). Since the conversion rate of each step of the method of the present invention is higher than 98%, it indicates that the method of the present invention is suitable for industrial production.